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By Ralph Sweetser

IN these days of the almost exclusive use of byproduct coke as the blast-furnace fuel in this country, it may seem out of place, and smacking too much of reminiscing, to say anything about the use of anthracite coal for blast-furnace fuel. Viewed in the light of present day research and of developments in alloy steel, some observations seem appropri-ate regarding this raw material that played such an important part in the development of the iron and steel industry during 50 years of the past century. The research work of that period, in which the whole iron and steel industry was revolutionized, passing from wrought iron to steel and from charcoal to three new mineral fuels for blast furnaces, was done chiefly in the full-sized plants of that day; and it was done largely by the ironmasters themselves. The laboratory had not become a part of the ironworks, and scientific instruments were lacking around the blast fur-naces; "rule o' thumb" and erroneous theories prevailed-and have not yet all been eliminated. The recent interest in meteoric iron in connec-tion with nickel steels and other alloys proves that it is worth while to search for the reasons for excellence and the causes for failures in the metallurgy of bygone days. Turner1 gives the reasons why the blast furnace of Dr. F. W. Geissen-hainer on Silver Creek, Schuylkill County, Pennsylvania, about 10 miles northeast of Pottsville, was operated successfully with anthracite2 in August and September, 1836, and why several other attempts failed. It has taken a long time for us to find out that there are great differences in the behavior of anthracites from the several parts of the anthracite region, as well as differences in coking coals from the bituminous fields.

Jan 1, 1935

By F. B. Foley

With the possible exception of high-speed tool steel, the service demanded of rock-drill steel is probably more precarious than that of any other tool steel. Unaided by the helpful influence of alloys and dependent solely on the efficiency of the heat treatment applied for its ability to stand up under the abuse to which it is necessarily subjected, rock-drill steel is worthy of intensive study. For its heat treatment the smith has his fire, an oil fire perhaps, and a quenching bath; he judges the temperature by his eye. There are shops where excellent drills are produced by this method, but there are more where the product varies between very good and very bad. Pyrometers with specially designed equipment are used in but few cases. But the responsibility for rock-drill failures does not rest entirely on the smith. Little has been published concerning the efficiency of drill steel, though the Canadian Mining Journal1 published the breakage record of a large number of hollow drill steels. This record indicates that most of the breaks occur during the early life of the steel and that as a given batch of steel is used, its percentage of breakage decreases. This fact, the article points out, is at variance with the much-talked-of theory concerning failure from crystallization and fatigue. It seems to point to the fact that the greater part of drill-steel failure from breakage is traceable to faulty manufacture, resulting in defects in the bore of the hollow steel from inclusions of slag or oxides, etc. As this defective material meets with early failure, it is weeded out. In addition, some breakage may be caused by a lack of proper condition with respect to heat treatment of the steel as furnished by the manufacturer. In the article mentioned, the breakage of 1/14-in (3.17 cm.) hollow steel is given as 4.62 per cent. for the early period of use, with a decrease to 3.35 per cent. and 2.67 per cent. with time in use. For 1-in. (2.5 cm.) hexagonal hollow steel, the figures for breakage are 0.18 per cent. and 0.06 per cent.; attention is called to the great decrease in breakage by the use of smaller diameter drills. The figures are given as so many drills sharpened, but there is no way of determining the percentage of

Jan 1, 1922

By Stanley C. Herold

A few hates on the occurrence and significance of mud volcanoes in Colombia may be of interest at the present time, owing to the renewed activity in geological exploration of the coastal regions bordering the Caribbean Sea. The best-known volcanoes are found a few miles from the seacoast. One is situated to the south of Puerto Colombia; the second, to the east of Cartagena near the village of Turbaco; and the third, near the village of Puerto Escondido south of the Sinu River. Others are reported in more inaccessible localities. Usually they stand 2 1/2 or 3 ft. (0.762 or 0.914 m.) above the surrounding ground at the crater, though several craters from 10 to 20 ft. -(3.04 to 6.09 m.) "apart will often build up an extensive mound at low gradient. The shallow mound may cover 1/2 or 3/4 acre (0.2 to 0.3 ha.) with an elevation of 12 or 15 ft. (3.65 or 4.57 m.) at the, center. The craters are formed of hardened blue clay; the inside diameters vary from 14 to 24 in. (35.56 to 60.96 cm.). The rim is continuous, except on one side where there is usually a cut 3 or 4 in. deep, thus allowing an overflow. The craters are filled to the' rim-cut with a thick mixture of blue clay mud and water, which is kept in agitation by escaping gas. Fig. 1 shows the bubble in the act of bursting and Fig. 2 the appearance of the surface of the viscous fluid a second or so later. The frequency of the explosions is determined by the weight of the column of fluid in the neck of the volcano, consequently, such explosions are not synchronous in a group of craters. Ordinarily, there arc two or three explosions in about 3 minutes. The supply of gas is small but steady and sufficient pressure must accumulate before the bubble can enter the column of fluid. The water is derived from the surface and enters the scdirnentary strata not far distant from the volcano. During long dry seasons, as the supply of water fails the volcano dries and geyser action ceases. The temperature of the muddy fluid is normal; the gas is dry and inflammable. - No petroleum products come with the gas. On the surface of the fluid, there is sometimes a dark brown streaky scum, which

Jan 1, 1920

By W. Z. Price

The coal lands that the Nemacolin mine is to develop embrace over 8400 acres; the tract is oblong and its eastern edge is along the Monon-gahela river. As shown in Fig. 1, the mine is divided into two parts (the North mine and the South mine) by a 150-ft. barrier, which however, is cut through at intervals by haulageways. Each part is fed from seven main entries—a loaded track, an empty, a manway, and four return air courses. The loaded tracks converge at the shaft bottom but the empty roads maintain their identity throughout their length. With three intakes and four returns on either side, there is ample room for expansion of air and every facility for ventilating is provided. The four south air courses converge into two, crossing the shaft bottom, and then into one at the south side of the air shaft. The four north air courses converge in a similar manner on the west side of the same shaft. This convergence is accomplished by concrete arched

Jan 1, 1927

By Frederik W. de Klerk

INTRODUCTION During the past 40 years, there has been in the United States of America and other industrialised Western countries a distinct displacement in the procurement of minerals from domestic sources towards an increased dependence on imported minerals. This was caused in part by one or each of the following: a lack of local supply of particular minerals, domestic source depletion or exhaustion and the relative ease and inexpensiveness of obtaining minerals from comparatively unexploited sources in underdeveloped and some developing countries, notably in the Middle East, South America, Southern Africa, and Australasia. Governments of the industrialised nations, concerned about the reliance of their economies on imported raw minerals examined both the degree of reliability and the extent of mineral resources in the countries and regions supplying the essential minerals. This brought a painful awareness of the vulnerability of industrialised countries as a result of the possible interruption of their mineral imports. In this regard, the United States of America may be quoted as a case in point: a report by a House of Representatives Subcommittee on Mines and Mining (Santini Subcommittee)1 revealed that the United States in 1980 was dependent on foreign sources for more than 50 per cent for 24 of the 32 minerals essential for national survival. The Subcommittee also acknowledged that although the United States may develop its own alternative energy sources, there are in many cases no substitutes for the strategic + minerals imported from foreign sources, from countries which are often unstable at best, hostile at worst. This resulted in various policy responses as well as contingency measures, amongst other, renewed emphasis on the utilisation of domestic mineral resources, an intensified search for substitutes of critical minerals and increased stockpiling programmes. Increased attention was devoted to analyses of the political and economic conditions prevailing in the regions from which strategic and other minerals are exported to the industrialised countries, and the formulation of policy measures vis-a-vis those regions. One region which attracted a considerable degree of attention has been Southern Africa, and in particular South Africa.2 The Santini Subcommittee affirmed that while the bulk of the minerals imported by the United States is supplied by a number of source countries, a host of critical[t] minerals vital to the well-being of that country (and this includes all the Western industrialised countries) originates from Southern Africa, a region, deservedly referred to as the "Persian Gulf of Minerals". Apart from the Republic of South Africa the mineral-rich countries concerned are Angola (diamonds, iron ore, oil), Botswana (diamonds, coal), South West Africa/Namibia (diamonds, uranium), Zambia (copper, cobalt), Zaire (industrial diamonds, copper, cobalt) and Zimbabwe (gold, nickel, chromium, asbestos). The Subcommittee however noted that, with the exception of cobalt, the greatest portion of the reserves of the critical minerals listed, lies within the borders of South Africa. SOUTH AFRICA A RELIABLE PURVEYOR OF MINERALS In view of the continual instability and political risk, along with the nationalisation of mineral industries in third world countries, importing industrialised nations have in recent years become more and more concerned about security of long-term supply, and have in consequence begun to diversify their mineral enquiries to areas where the following conditions prevail: • Long-standing record of consistency of supply; • An economic system of private enterprise; • Political stability; • A well integrated infrastructure, with a maintenance of transportation and development costs at realistic levels, and • Attractive investment opportunities, with security of the return of profits.

Jan 1, 1982

By S. R. Mitchell, M. C. Fuerstenau, A. M. Gaudin

The two principal attributes of a thickener pulp are its settling rate and the ultimate pulp density of the thickened mud. Testing for evaluation of thickening attributes of a pulp has usually been done batch-wise by placing the pulp in a one-liter glass graduated cylinder and noting the position of the boundary between clear liquor and mud as a function of time. Refinements in testing have included repulping a thickened mud to various dilutions and evaluating the settling rate on these various repulped muds. This is considered to make possible an estimate of the settling rate as a function of pulp density and therefore to pinpoint the slowest settling pulp which ought to be critical from the standpoint of thickener plant design. Finally, tests are sometimes made with model-size continuous thickeners of arbitrary size. In batch tests it is generally accepted that the behavior of a pulp is described by a curve such as the one shown in Fig. 1, in which the position of the boundary between clear liquor and mud (the mudline) is plotted against time. It has also been assumed that the initial settling rate (the slope of the line segment AB) is descriptive of the pulp and independent of the size and shape of the container. Where the settling rate is slower and clearly a function of time (portion CD of the settling curve), it has been assumed that the data are not of much use because of the intrusion of compacting phenomena. The next important datum is the height, PE, which is a measure of the so-called ultimate pulp density. This quantity is assumed to be characteristic of the pulp and independent of the container.

Jan 6, 1959

By M. P. Boss

Of the two methods of mechanical reduction—that of percussion and that of abrasion—it is not easy to say which was first employed by primeval man. The stone hammer and the flat or hollowed stone used for grinding are found together in the remains of prehistoric periods. But the use of the maray, or bucking-stone, developed from the hammer, was probably introduced later than that of crude millstones. Diodorus Siculus, the Roman historian of the first century B. c., mentions such millstones as used in the mines of Egypt to pulverize material which had been previously broken in a mortar. The invention of the arrastra for fine grinding is declared by some authorities to have been made by Bartolomeo de Medina, at Pachuca, Mexico, about A. D. 1557—which is quite probable. Being the first to amalgamate silver on anything like a business scale, he must have felt the necessity for oregrinding apparatus of greater capacity than the old primitive millstones; and the arrastra was thus the natural successor of the millstone. It is very unfortunate that the archives of Pachuca, which has made so much history in ore-treatment, were destroyed in some one of the many insurrections for which, also, the place is renowned. The first application of the stamp to the crushing of rock is asserted by some writers to have been the invention of a Saxon nobleman named Von Maltitz, about the year 1505. Better authenticated reference, however, is made to one Paul Gronstetter, a native of Schwarz, and called an ingenious worker, who, in the year 1519, established at Joachimsthal a process of wet stamping and sifting. Two years later, a larger plant was established at the came place. It is said that he had previously introduced the same device at Schneeberg. How much of the invention was due to Gronstetter is not certain;

Jan 1, 1902

By W. H. Gunniss

When the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of an average sample of this quartz is: SiO2, 96.7; Fe2O3, 0.3; Al208, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then dumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left. until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected to when in use in the furnaces. Montana refractories are used in smelters throughout the West. Prospecting for fire clays was also carried on. After experimenting with clays from several different deposits, it was found that a mixture of

Jan 1, 1914

By L. E. Welch, C. W. MacGregor

THE past 20 years has seen a revolutionary change in the testing of materials at elevated temperatures. This has largely been brought about by the practical importance of the creep problem in the design of equipment for operation at high temperatures. The short-time tension test carried out at elevated temperatures has consequently assumed in many cases only a secondary role compared to the long-time creep test. In many problems, however, a knowledge of the short-time high-temperature properties of a metal is essential. To mention a few cases in which this is so, we might include all hot-forming operations such as rolling, forging, etc., the welding problem if residual stresses are to be computed, the development of new alloys for high-temperature service where, in the initial stages, time does not permit of long duration creep tests, and others. Usually a knowledge of the short-time properties is desired, if only to serve as a background against which to compare creep behavior. In conducting short-time high-temperature tests, it has been almost the universal practice to determine stresses based on the original area and strains referred to the original gauge length which is usually chosen as 2 in. It has been pointed out 1,2 that one of the reasons that the true significance of certain tensile properties is not understood, which perhaps curtails their usefulness, especially when the material is applied [ ] under conditions differing considerably from the test conditions, is that true physical stresses and strains are not determined. It is essential to have a knowledge of true stresses and strains in order to correlate the values present in the tension test with those existing, for example, in hot metal-forming operations and in the general problem of the yielding and failure of metals under combined stress conditions. Stress and strain values based on the original dimensions of the test piece do not exist physically except in the early stages of the test. Since at the present time there is very little information in the literature on true stress-strain relations in the short-time high-temperature tension test it is proposed in the following pages to describe a

Jan 1, 1942

By M. D. Arnold, H. J. Gonzalez, P. B. Crawford

A method is presented for estimating the effective directional permeability ratio and the direction of maximum and minimum permeabilities in anisotropic oil reservoirs. The method is based on the principle that production from a well in an anisotropic reservoir results in elliptical isopo-tentials about the well, rather than circular. Bottom-hole pressure data from three observation wells surrounding a producing well are required to apply the method. The method involves fitting field pressure data to a set of general charts of isopotentials and making a few simple calculations until a solution is found. The method is based on a steady-state equation for homogeneorrs fluid pow. In addition to the method, a brief discussion of the theory underlying it is presented. INTRODUCTION The existence of a different permeability in one direction than another in oil reservoirs has been mentioned in several papers. Hutchinson' reported laboratory tests on 10 limestone cores and pointed out that one-half of them showed significant, preferential, directional permeability ratios, the average being about 16:1. Johnson and Hughesz reported a permeability trend in the Bradford field in the northeast-southwest direction with flow being 25 to 30 per cent greater in that direction. Barfield, Jordan and Moore -eported an effective permeability ratio of 144:1 in the Spraberry. Crawford and Landrum4 showed that sweep efficiencies could often vary by a factor of two to four, and sometimes considerably more, due to variations in flooding direction and patterns in anisotropic media. These findings indicate that the poss'bility of anisotropy may be worthy of consideration in the development of an oil field. In considering this, it should first be determined if anisotropy exists. If it does, the direction of the maximum and minimum permeabilities and the ratio of their magnitudes are quantities which can be of value in planning the most efficient well-spacing patterns. Past methods of determining these quantities have included analysis of oriented cores and analysis of flooding performance of pilot injection patterns. In recent work, Elkins and Skov5 resented an analysis of the pressure behavior in the Spraberry which accounted for anisotropic permeability. This work was based on the transient pres- sure distribution in a porous and permeable medium, with the solution expressed as an exponential integral function involving rock and fluid properties. The purpose of this study is to provide a method, based on steady-state equations, of estimating the direction and relative magnitude of permeabilities in an oil reservoir from field pressure data and well locations only. The method presented is based on work by Muskat6 which shows that Laplace's equation represents the steady-state pressure distribution for homogeneous fluid flow in homogeneous, anisotropic media if the co-ordinates of the system are shrunk or expanded by replacing x with it is desirable that data be obtained early in the history of a field because knowledge of an anisotropic condition would allow new wells to be spaced in such a manner that reservoir development and subsequent secondary recovery programs could be planned more efficiently. THEORETICAL CONSIDERATIONS A brief discussion of the theoretical basis on which the graphical solution was developed is presented in this section. Muskat's two-dimensional6 olution for the pressure distribution in an homogeneous, anisotropic medium with an homogeneous fluid flowing can be algebraically manipulated to show that the isobaric lines are perfect ellipses. The ratio of the major axis to the minor axis, a/b, is related to the permeability ratio, k,/k,, as follows. alb = dk,/k,--...........(1) It can also be shown that the pressure varies linearly with the logarithm of the radial distance from the producing well. However, the gradient along any ray is a function of the orientation of that ray, and a ..xiable is present when anisotropy exists which cancels out for a radial (isotropic) system. For a system such as that described, a dimensionless pressure-drop ratio was developed which is completely independent of the actual magnitude of the pressures. This was done by arranging Muskat's solution in such a way that aIl variables cancelled out except k,/k, and well positions. However, this solution depends on having a co-ordinate system with axes coinciding with the major and minor axes of the elliptical isobars. Thus, it was necessary to introduce a co-ordinate system rotation factor. The two unknown variables are then k,/k. and 0, and the two measured dimensionless pressure-drop ratios are related to the unknown variables as follows.

By M. F. McCarty, R. S. Olson

New organic flocculants of high-molecular weight are replacing lime, glue, and starch in liquid-solid separation. Of these synthetic materials, poly-acrylamides are outstanding. Polyacrylamides form a class of compounds varying widely in composition and activity. Separan 2610, one of the first of these flocculants' released to the mining industry in 1954, is described' as a high-molecular weight polymer of acrylamide with or without a copolymer material and with some replacement of amide by carboxylic groups. MECHANISM OF FLOCCULATION In practice, flocculation makes solids settle faster and filter better. But two opposing factors control it. The random motion that causes particles to collide favors Van der Waals' forces, which hold the particles together. The effect of zeta potential opposes this contact, and particles are mutually repelled. Flocculation can be achieved by reducing the magnitude of the zeta potential; this is the mechanism of flocculation by lime addition. The way in which polyacrylamides accomplish flocculation is not fully understood, but the action is undoubtedly comp1ex and probably varies considerably depending on the system. To begin with, the active groups of these compounds have an extremely high affinity for solid surfaces, probably by hydrogen bonding." Initially some active groups of the molecule attach themselves to the solids with a large portion of the molecule extending into the solution. Two particles can become tied together by long flocculant molecules in the following ways—by bonding between the active groups of two flocculant molecules on different particles, or by an extended molecule from one particle attaching itself directly to the surface of the other particles." These flocculant bridges prevent the particles from moving apart through random motion, but when such motion moves them together other active groups on the flocculant bridge bond to the solids, holding them in the closer position. This process is repeated until the particles are close together. Although bridging is probably a major flocculation mechanism, it is not the only phenomenon involved. Relatively neutral acrylamide flocculants reduce the magnitude of the zeta potential by increasing the viscosity of solution in the immediate vicinity of the solid surface which contains the mobile counter ions of the double layer. In other words, it moves the shear surface which bounds the zeta potential out into the solution containing counter ions which tend to neutralize the zeta potential. This effect is probably more pronounced during the initial adsorption period, before the flocculant molecules are pulled close to the solid. In some cases the slight charge of the polyacry-lamide molecule tends to neutralize a zeta potential. However, this is not a primary flocculation mechanism, as evidenced by the fact that the polyacrylamides will flocculate solids with either positive or negative zeta potential. Adsorption of polyacrylamide flocculants by a solid is substantially an irreversible reaction. Since the flocculant molecule is attached to the particle surface by many active groups of high bonding strength, desorption would require the simultaneous breaking of many bonds—an unlikely occurrence. UNIQUE PROPERTIES The irreversible adsorption of certain polyacrylamides, the flocculant's high affinity for solid surfaces and its rapid adsorption make it effective, but these unique properties require special techniques to achieve maximum flocculation. If flocculants of this type are added to a pulp as a relatively concentrated solution, the solids in the

Jan 1, 1960

By W. L. Falke, A. A. Cochran

A basic problem in connection with manganese is to find economical ways to utilize domestic resources. As a part of its program to conserve domestic mineral resources and to reduce dependence of foreign sources, the Bureau of Mines had conducted extensive research to broaden manganese technology and to find economical, technically-feasible processes for recovering manganese from these low-grade resources. This paper analyzes some of the major difficulties which have been encountered in previously proposed processes for treating low-grade manganese ores and discusses a process which may circumvent many of these difficulties. Vast deposits of low-grade manganese ore exist in the U.S., yet domestic production is insignificant compared to the more than 2 million tons of ore imported yearly into this country.' A basic problem in connection with manganese is to find economical ways to utilize domestic resources.2 As a part of its program to conserve domestic mineral resources and to reduce dependence on foreign sources, the Bureau of Mines has conducted extensive research to broaden manganese technology and to find economical, technically feasible processes for recovering manganese from these low-grade resources. Although a great many processes have been proposed for treating domestic manganese resources, a failing of many of them is that too many steps are involved for economical operation.' Some of the major processes that have been proposed were reviewed by Norman and Kirby.3,4 Chlorination processes have become increasingly useful as a means of recovering valuable metals from raw materials, because the relative cost of chlorine (Cl2) and hydrogen chloride (HC1) has decreased through the years, and because the corrosion resistance of materials of construction has been improved. The objective of these processes is to form metal chlorides that are more volatile or water-soluble than are the corresponding oxides or sulfides; these compounds then can be separated from the gangue or other minerals by volatilization or leaching. Several chlorination processes for the recovery of manganese have been investigated by the Bureau of Mines5-8 and others; the major chlorination processes were reviewed in 1963, and their main features were compared.4 In all these processes, the simultaneous leaching or volatilization of iron chlorides with manganese chloride (MnCl2) is a problem, and the more iron that is present, generally the greater the problem. The leaching step is not highly selective, and the product of this step is, at best, suitable only for the production of ferromanganese or for further processing to remove iron. The product of the volatilization step is, in all cases, a mixture of iron and manganese chlorides that contains too much iron even for ferromanganese production, and must undergo additional processing steps for iron removal. THERMODYNAMIC CONSIDERATIONS The literature indicates that the desired chlorination reactions will proceed at practical rates at temperatures near 1200°K (927°C). Free energy changes at 1200°K for the critical steps of the reduction and chlorination reactions9-11 follow: Most of the research on chlorination processes for manganese recovery has been done with HC1 rather than with C12, for the following three main reasons: 1) Recycling of the chlorinating agent, which is economically vital, appeared to be easier for HC1

Jan 1, 1968

By K. D. Hester, A. W. Fletcher

A nickel-copper sulphide concentrate was treated in a pilot plant at Warren Spring Laboratory during 1961, by a hydrometallurgical roast-leach-solvent extraction process devised to cleanly separate the metal values and produce acid sulphate liquors containing the metals. It is shown that 86 pct of the nickel and 95 pct of the copper could be leached from the calcine, after a sulphatizing roast on finely ground flotation concentrate. Iron was removed from the leach liquor by limestone neutralization with a small loss of values. Copper and nickel were separated by solvent extraction with naphthenic acid in kerosene after partial neutralization of the iron-free liquors with ammonium hydroxide. Hydrogen sulphide and chlorine were used to remove zinc (and residual copper) and cobalt impurities respectively. The recovery of pure copper and pure nickel, by electrowinning, from the acidic solvent extract strip liquors finally produced, appears technically feasible. An economic analysis of production costs shows that small, geographically isolated, nickel-copper sulphide deposits cannot usually be worked profitably by established processes. The requirements for profitable operation on a comparatively small scale could possibly be met by a flotation-roast-leach process. Two difficulties, obtaining satisfactory extraction of nickel from a sulphide concentrate and separating the copper and nickel in solution, have prevented the previous use of this method. A solution to the first problem, dissolution of the nickel, was described in a recent paper by Thornhill.1 It was shown in this paper that copper and nickel in a flotation concentrate could be oxidized to water soluble sulphates by roasting in a fluidized bed with added salt cake. Workers at the Warren Spring Laboratory have shown that the separation of copper and nickel can be accomplished by solvent extraction using a relatively inexpensive carboxylic acid, naphthenic acid. Moreover, the mineral acid required to strip values from the loaded solvent could be produced, and the metals recovered, by electrowinning; thus the latter section of the process was regenerative. The removal of iron from the leach liquor and the elimination of impurities such as zinc and cobalt before nickel electrowinning would be necessary to complete the flowsheet. The process under investigation could therefore be summarized (Fig. 1) as follows: 1) Flotation to produce a bulk sulphide concentrate. 2) Fluidized bed roasting to sulphate the nickel and copper minerals. 3) Leaching of roaster calcine to extract soluble nickel and copper. 4) Precipitation of iron from the separated leach liquor by air oxidation after the adjustment of pH and temperature. 5) Recovery of copper from the iron-free Liquor by pH adjustment and liquid-liquid extraction. 6) Purification of the copper raffinate by removing zinc and residual copper as insoluble sulphides and cobalt as cobaltic hydroxide. 7) Recovery of nickel from the purified liquor by pH adjustment and liquid-liquid extraction. Laboratory and pilot plant studies detailed below, were carried out at the Warren Spring Laboratory, to test the feasibility of each one of the unit processes and to obtain preliminary plant design data. FLOTATION The ore was an altered basic rock containing concentrations of magmatic sulphides.

Jan 1, 1964

By N. E. Rogen, N. J. Grant

WHILE direct measurements of the growth of precipitate particles during aging is of fundamental value, few such measurements have been made. Direct measurements by means of optical or electron-microscopy and X-ray techniques are preferred, however, many of the aging studies have been based on indirect methods such as electrical resistivity and hardness. Because of the minute size of most precipitate particles (less than 1000A) the light microscope is of limited use while electron microscopy is subject to slowness, etching problems and consequent resolution problems. It is fortunate that alloys of the Nimonic type, based on Ni-Cr-Ti-Al, lend themselves to accurate and relatively easy particle size measurements. With proper balance of titanium and aluminum, the only aging precipitate is the gamma prime (r') Ni3,(Al, Ti)2 phase and this phase is the basis of the high-temperature strength of these allos.3-6 The Ni3(Al, Ti) phase is a face-centered-cubic, ordered structure with nickel atoms occupying the cube faces. Titanium atoms can replace three out of every five aluminum atoms and when substituting do so preferentially.2 Electron microscopy has shown that during aging of most of the commercial alloys of this type, precipitate particles are unusually uniform in size and distribution, and that the volume of (r') phase is large (20 pct).4,7 The aim of this investigation was to measure the growth of (y') phase during aging. In so doing, it was hoped that a clearer understanding of the aging process would be attained. X-ray line broadening was used as the measure of precipitate particle size. This technique was selected because it can measure and average the diameter of thousands of particles in one operation. The variations in hardness and matrix lattice parameter with aging were also studied and related to the particle size. EXPERIMENTAL PROCEDURE An alloy of the following composition was studied: Cr Ti A1 C Ni Wt pct 20.71 2.98 1.43 0.04 bal. At. pct 22.06 3.47 2.95 0.18 bal. The alloy, a 15- lb vacuum melt, was forged to 1/2-in. diam at a temperature of 1900" to 2200°F; was solution heat treated for 4 hr at 2000°F and water quenched; and was then aged in various ways. The ASTM grain size was 4 to 5. No (7') phase could be detected by X-ray analysis after solution treatment and electrolytic extraction. Aging was performed on 2-in. long specimens at 1400°, 1500°, and 1600°F for increasing times. One-half inch sections were removed after each time increment and were then electropolished in a solution of H3P04 saturated with chromium trioxide at a potential of 30 v and rectified with a tantalum electrode. Rockwell hardness measurements were taken using one side of the polished specimen. Matrix lattice parameter determinations were made on the other side using filtered chromium radiation references with the position of the (220) line of a silicon standard. To enable the precipitate particles of the (y') phase to be measured using X-ray line broadening techniques, it is first necessary to separate and concentrate this phase by electrolytic extraction. Extraction is necessary because the difference between matrix and precipitate lattice parameters is only approximately 0.5 pct and intensities of.the (y') phase lines are very weak relative to those of the matrix. The extraction techniques employed have been described before and found to produce a reasonably quantitative separation.398 A water solution of 15 pct H3Po4 is used at a current density of 0.5 amp per sq in. at 6 v. The precipitate particles are separated from the liquor by centrifuging and decanting and are then washed, dried and repowdered. A plot of the X-ray intensity vs diffraction angle for the (111) line of the precipitate particles was used as a measure of particle size. The intensity curve approximated the shape of Gaussian distribution function and its breadth was measured at the half height. The (220) line of a silicon standard was used to correct the measured line breadth for instrumental and other broadening errors. The Scherrer formula was used to calculate particle

Jan 1, 1961

By Paul D. Merica

One of the most useful, and at the same time least commonly used, methods of thermal analysis for the determination of transformations in metals and alloys consists in the recording of the time intervals required for successive increments of temperature change during heating or cooling, the temperature of the furnace containing the specimen being altered at a uniform rate. The curve obtained by plotting these time intervals as a function of the mean temperature of the specimen durnig the interval is called the inverse-rate curve. It is probably due to the fact that no simple and convenient method has apparently been available for the measurement of the successive time intervals that this method has not been so generally used as, for example, the differential method, for which several types of automatic or semi-automatic apparatus have been designed. Whenever this method has been used, the intervals have usually been measured with the use of a chronograph; its operation as practised at the Bureau of Standards1 is as follows: The temperature of the specimen is measured by a thermocouple and a dial potentiometer. The operator sets the potentiometer at successive values of the electromotive force differing by equal increments, usually 0.02 millivolt, and records the exact instant on the chronograph, by pressing a contact key, at which the galvanometer coil passes through its null position. Two-second intervals are also recorded on the chronograph record, and the number of seconds elapsing between successive signals is afterward counted from the record and plotted as a function of the electromotive force or of the temperature. This is an admirable method and by it most minute thermal arrests may be detected, but it requires a good chronograph, which is generally difficult to obtain, and the time of one operator during the recording and, subsequently, to read the intervals from the record; the latter operation often takes from one to two hours. There is here suggested a simple, convenient, and, it is believed, equally accurate method of recording the successive time intervals, by which the

Jan 1, 1921

By Benj. E. Shackelford

THE present paper is concerned with typical temperature values experienced in lamp-filament measurements as made on regular factory and engineering products. It deals with the relations existing between temperature, efficiency, lamp size, and life of incandescent lamps, insofar as they affect the rating of the product and its use by the individual consumer. The temperatures measured lie in that range covered only by the general method of radiation pyrometry, as opposed to direct methods used under contact conditions. The range of temperatures ordinarily experienced extends from about 2125° K., for the now almost extinct carbon-filament lamp, to 3200° K. for the comparatively new tungsten-filament motion-picture lamp. Most of the more common sizes of tungsten lamps have temperatures ranging from 2500 to 3000° K. Because of the high temperatures involved and the relatively small area of the sources used, we are practically restricted to two methods of measurement, both of which depend on the light radiated front the filament. The first and more usual method is that of the Morse pyrometer, dependent on the variation in temperature of the amount of light of a given color range yielded by the filament. In this case, the measured temperature is that of a small part of the incandescent body, that is, the part which is focused on the comparison filament. The second method, known usually in this country as that of "color match" and in England as "color-identity" is based on the color of the total light yielded by the filament, the comparison being facilitated by the use of an ordinary photometer- head. A more definite idea of the temperatures involved in the case of filaments of various vacuum and gas-filled lamps, is given by Fig. 1. The size of the lamp, in watts, is plotted along the horizontal axis and the temperature of the filament is plotted along the vertical axis. The lamps concerned are regular product, rated for 1000 hr. life. The temperature values for the old 16-candlepower carbon lamp and the new motion-picture lamp are shown by the cross and circle respectively.

Jan 9, 1919

By M. A. Rigdon, R. E. Grace

The dissociation of cupric oxide to cuprous oxide and oxygen was studied with a microbalmce technique at 700" to 750°C. In this temperature range the dissociation pressure of the reaction 2CuO= Cu2O + 1/2 O2 was: The theory of near-equilibriwm reaction rates predicts a linear relationship between reaction rate and the Gibbs free-energy change for small values of AF/RT. This correlation is found to be valid for AF/RT = -0.1 or approximately 200 cal per mole away from equilibrium. THE theory of reaction rates near equilibrium as developed from classical thermodynamics suggests a small range of linear behavior between the overall reaction rate and the free-energy change accompanying the process. The extent of this linear correlation is generally unknown, even to the order of magnitude. The idea of linearity is also found in the formal mathematics of coupled transport phenomena, e.g., chemical diffusion, thermal diffusion, thermoelectricity, and so forth. The linear array of forces and fluxes which leads to various main and cross coefficients is predicated upon linearity between reaction rates and the bulk thermodynamics which govern the process. The general case in reaction kinetics is well-known: the magnitude of the free-energy change does not cor- relate with observed reaction kinetics, irrespective of whether the process occurs by diffusion or chemical reaction or both. The real need is to investigate specific reaction paths near equilibrium in order to learn of the limitations in attempting to correlate reaction rates and thermodynamics. It is the main purpose of this paper to examine the dissociation kinetics of cupric oxide under conditions of known driving force where the dissociation process is likely to occur by chemical reaction. A secondary objective is to obtain equilibrium data for the CuO-Cu20-O2 system. In a prior paper Edmiston and race' investigated reduction kinetics of wustite in H2-H2O gas mixtures. The present study was carried out in oxygen according to the following reaction:

Jan 1, 1969

By A. K. Knickerbocker

PRACTICALLY all underground work on the Minnesota iron ranges is done by miners working on a so-called contract wage system. This system, while it has certain advantages over the straight day's pay or company-account method of wage payment, has serious and vital defects. In view of the scarcity and demands of labor, it is important that employers of labor scrutinize their systems of wage payments carefully, not only to save losses and trouble, due to labor disturbances, but also to secure the greatest efficiency of their workmen and reduce their operating costs. It is admitted that an adequate, just, and equitable wage is the prime factor in bringing about these benefits. The wage of labor and its method of application and payment have been, and always will be, the main factors in the unrest and dissatisfaction of labor. Not only does labor want and need an adequate wage, assuming that work is adequately performed, but it wants and is entitled to a just and equitable wage. Labor must have respect for the fairness of the wage and for the fairness of the management in the application of the wage. It is conceded that the Minnesota iron miners are now, and have been, in the main paid adequately, but the inherent defects of the so-called contract system prevent any just or equitable application of this wage to the various units of the labor body. The defects of the contract system, with its obvious inequalities, favoritisms, and injustices, are cancers in the brain of labor. Every thinking miner realizes these defects and knows just what they are; the unthinking do not realize the details of the subject, but each month they are forcibly reminded of these defects through the pay envelope. As practiced on the iron ranges, however, the so-called." contract" system is not a contract and the name is a misnomer. No true contractual obligation exists.

Jan 2, 1920

By Eugene E. Ayres

The centrifuge has come into general use in the oil fields and in the establishments where lubricating and fuel oils are used. Probably centrifugal machinery will be found more useful in the refinery when the operators are more familiar with'the principles of modern centrifuga-tion and when centrifugal engineers better understand the refinery emulsion problems. It is not generally realized that centrifugal force and gravity have two distinct functions: First, subsidence wherein the suspended globules are brought into contact; second, coalescence (when this is possible) by rupturing the films around the globules. In the case of a water-in-oil emulsion, an exercise of the former function alone would yield: (1) oil, free, or as free as desired, from water; and (2) a concentrated water-in-oil emulsion—concentrated in the sense that it contains a relatively large percentage of the internal phase. An exercise of both functions will yield: (1) water-free oil and (2) oil-free water. Centrifugal force is much better than gravity for subsidence because, in the case of industrial emulsions where the suspended globules are visible under a microscope, subsidence is directly proportional to the force applied. Centrifugal force is only slightly better than gravity for coalescence. A minute trace of a proper reagent will immediately do more to nullify the interfacial surface tension opposing coalescence than an indefinite application of the highest attainable centrifugal force. No mathematical analysis has been made to explain the failure of high centrifugal force to induce a decidedly more rapid and more complete coalescence than is obtained by gravity. The adjustment of the centrifuge rotor depends more on the extent of coalescence that is desired or is possible than on any other factor. One reason for this dependence is to be found in the curious relation between the specific gravity and the hydrostatic pressure of emulsions. The continuous centrifuge works on the U-tube or Florentine flask prin-

Jan 1, 1924

By H. W. Mead, C. E. Birchenall

SELF-DIFFUSION in pure gold has been studied by Sagrubsky,1 McKay,2 Gatos and coworkers,3,4 and Okkerse.5 Sagrubsky used a sectioning technique but reported results far lower than any of the others. The work seems to be carefully done, and it appears that a factor of 60 must have been omitted in his calculations or the units misstated by an equivalent amount. McKay used a surface activity method, and Gatos and Kurtz, following Gatos and Azzam, applied autoradiography to the measurement of activity on an oblique section through the diffusion zone. These two investigations agree well with each other but give results below those reported here. Okkerse employed a very careful sectioning technique. Chemical interdiffusion in Au-Ag alloys has been measured under several concentration conditions. Average values of the diffusion coefficient for the range of 0 to 18 atomic pct Au were obtained by Braune.6 since the diffusion coefficient probably varies markedly over this range, the values may not be too useful. Also, a plot of these data suggests that grain boundary contributions may have been appreciable at the lowest temperature employed. Ebert and Trommsdorf7 give average values for 0 to 9 atomic pct Ag, and Johnson8 reports average values for 45 to 55 atomic pct Au. Johnson also measured silver and gold self-diffusion coefficients in 49.2 atomic pct Au alloys, and self-diffusion in pure silver. The self-diffusion of gold in pure silver has been determined by Jaumot and Sawatsky.10 Other measurements which do not cover a range of temperature or are of low precision are not mentioned in this account since a review by Kubaschewski is available." This contribution reports diffusion coefficients for self-diffusion in gold, self-diffusion of gold in Au-Ag alloys, and chemical diffusion in Au-Ag alloys. Although it had been intended to obtain silver self-diffusion data in the alloys it now appears unlikely that these measurements can be done soon, so a table has been worked out for a self-consistent scheme of diffusion coefficients which should not be too far from the true values. Experimental Details Experiments on pure metals were conducted using fine gold of 99.99+ pct Au and silver of the same purity. Alloys were prepared by melting the two metals together in a graphite crucible in vacuo and allowing the slug to solidify in the crucible. After machining to a cylinder about 0.85 in. diam each slug formed one half of a diffusion couple. Compositions were determined later by analyzing chips taken from the extremities of the diffusion zones. The gold used in the preparation of alloys was sometimes pure gold but was normally either in the form of clean pickled alloy from previous experiments or gold recovered by oxalic acid precipitation from warm aqueous solution. Chips from the various stages of experimentation were dissolved in aqua regia and the solution taken to low bulk, diluted with water, and again taken to low bulk before diluting for the precipitation. This precipitated gold contained a small amount of silver as the only impurity detectable by spectrographic analysis. Disks for use in diffusion couples had opposite plane faces abraded on emery paper as far as zero grit, were annealed for 12 hr at 900°C in argon, and had one face of each disk polished to 000 emery paper. Radioactive gold was plated at about 2 ma per sq cm from a small volume of cyanide solution containing 1 mg of inactive gold as a carrier. Specimens , were freshly abraded on 4/0 emery paper immediately prior to plating. In the case of the active couples disks of a similarly prepared but unplated alloy or pure metal were placed on top and welded to the active disk. With the concentration couples disks of different compositions were welded. Welding was performed after a pressure of 5,000 lb had been applied at

Jan 1, 1958